Treatment of sugar-containing liquids



Patented May 11, 1948 mm' 1. Naugle, New

I mesne assignments, of

CorporatlomNew York, N. 1,". door- 7 l. r I

poration of New Yor o Ourv present invention odorization of cane and other sugar-bearing plant Juices, fruit Juices, raw sugar melts, and' washed Ij raw sugar melts, and constitutes a continuationin-part oi the co-pending application of John J.

Naugle entitled Treatment of sugar solutions,

Serial No. 543,423,-'flled July 3, 1944, nowPatent 2,422,699. I

flcation of the above-named liquids hadfbefore been accomplished by dei'ecation with'lime'; but

relates to the-treatment; oi s r-containing liquids, and more particu-j II larly, to the purification, decolorizatiomand demlnican sslescornomtlommwl oramm. f

ammmthn y? .I I A No Application Apr-n13, 19

k, and; mamas woun juid'fwitii panama, u ue abiei and ever. w ei ha e i frbl at n; n

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cordancewiththeiolloviring: ,I e; w n' d ta ght by wa r-a as J adefecantfor raw sugar .juice' solu'tionahas a caustic eil'ecton said solutions," gives low filtering i1! As stated in said co-pending application, clari-,

and causes darkening" 1 of; the defecated Juice. This "seeming disadvantage notwithstand- 1118, it appears that when calcium oxideis mixed such clarification had been found lacking in that the colloidalmaterials', gums, waxes, and other color and odor-imparting substances" normally present in such liquids were not removed to a suiilcient degree. Furthermore, such clarification required elevation of the temperature =01 the liquid to a point which resulted in undue darkening; the normal ash content of the liquid was increased; and tion rate. I i

In order to eliminate these disadvantages, the above-mentioned applicant proposed a double defecation process following: I

To the sugar-containing liquids to which reference has been made, headded from about 1%. to about 3%, based on the weight of the total 30 the muds thereof had a low illtra-- which, briefly, consisted of the i I I I I I I Y I use of'magnesium'oxideas.apunfyinga ent requires that the *su'gar -containihg] liquid being with magnesium oxide inthe proportions] of from aboutwparts-of calcium oxide orhydroxide and 70 parts of'nias'nesium oxide toiz'l, and the combination is utilized-inia process quite similar to that set forth in the' co pending application above referred to, we obtain, wi'th. about one-half the amount of defecant', results comparable to those sugar solids initially present, of a combination of 7 I the oxide and. hydroxide of an alkaline earth metal. such as magnesium. Breferably, the" hydroxide in the combination constituted about 2% thereof, although as high as 35% could bet'olerated, depending upon the nature of the starting sugar-containing liquid and the required of the end product, I

- After adding said oxide-hydroxide mixture. the liquid was heated to from about flTdeg-rees to about 79 degrees C. The heated liquid was settled and decanted, and the filtered.

precipitates were degree of purity' insolublesalts; 'as"well obtained when using the magne ium "oiddealone, and at a lower cost. Colloidal bodies, soluble and other suspended and "dissolvedimpurlties are'removed.

a While we ddhotwish to be restrictedto any particular theory a's't'o why this sliperiorresult is dition,--the'additio n of the calcium oxide relieves t the magnesium oxide of this burden, itself rais-' ing the pH to the proper value,*and permitting obtained, we believe that inasmuch as theefllcient treated'have a pH of about 9.7, and that when is actually wasted in attaining this alkaline conthe magnesium oxide 'to' devote itself more readily to'the task of purification and 'decolori'zation. We further believe that when' the calcium oxide does-not exceed '50 "ofxthe' mixture, the magnet siunio'xide' acts-as a protecting medium; and pre- The pH of a liquid so treated was about 10.00,

or slightly below. In order to bring thejjliquid substantially to neutrality, and to precipitate'im purities therein, forexample, as phos hat a gReferring now more indetail to .themanner 10% phosphoric acid solution was add'ed in an amount sufiicient to attain said substantial'neutrality. The liquid was then heated to about 83 degrees 0., after which it was permitted to settle. The clear liquid was drawn oil, and the muds filtered.

in whichwe avail ourselves of the above findings,

vents caustic action on the liq1'1id Whatever; the explanation, the end "product is far superior to any heretofore obtained .by' lime defecation, the muds have an unusually high rate of filtration, the ash content is 'considerablyreduced', and all these desirable results are obtained with fardess defecant than is possible .when magnesium oxide is used alone.

we proceed by first preparingthe magnesium oxide, Because this material readily absorbs moisture and carbondioxide and. for bestyr esults,

I I w, should beu'sed dry and practicaHyfree'otcarbon The endproduct oi'the foregoing wasa purified, clear, brilliant, light straw-colored liq dioxidait'is'preferred that the preparation thereor take place as near before using as possible.

The magnesium oxide may be obtained by calclning the hydroxide or the carbonate recovered from magnesite, serpentine, and other silicatebearing rocks; also, from dolomite, and from sea water.

While not limited thereto, the calcium-magnesium blend can be prepared by one of the fol-- liquid obtained from the decanting. This completes the first defecation. 1

It is now necessary to reduce the pH of the defecated liquid, which is about 10.00, substantially to neutrality. It is also necessary to precipltate therefrom impurities, for example, in the form of phosphates, or other insoluble comlowing methods, which are given by way of example only.

Ezample 1.When dolomite limestone is cal- ,cined, the resulting mixture of magnesium and calcium oxides occurs roughly in the proportions of one part magnesium to two parts calcium, the exact proportions varying with different limestones. Such a mixture of oxides is, for our purpose, too rich in lime. Therefore, in order to prepare a mixture of oxides containing the desired proportion of magnesium oxide, we mix with the limestone, prior to calcining, suiiicient magnesite (native magnesium carbonate) to give from about pounds. For these purposes, a 10% solution of phosphoric acid, or any other solution capable of reducing the pH and producing insoluble precipltates, is added in an amount suflicient to lower 50% to about 70% of the calcined mixture in the form oi magnesia. After calcination, the oxides exist in a rather'heavy form, having relatively little activity for decolorizing and purifying sugar any magnesia which goes into solution is recovered by boiling. The resulting light magnesium carbonate is filtered oil, dried and calcined, yielding an active magnesium oxide. To this oxide is now added the desired proportion of freshly calcined calcium oxide, ground until it passes through 200 mesh. The two oxides are thoroughly mixed and are ready for use. In place of powdered calcium oxide, calcium hydrate may the pH to from about 7.3 to about 6.9. The liquid is heated to about 83 degrees 0., and is permitted to settle. The clear liquid is drawn oil. and the muds are filtered, thus completing the second defecation.

' The resulting end product is an unexpectedly clear, brilliant and light colored sugar-containing liquid, which is remarkably free of-odor, and possesses a pleasant malt-like flavor. Sugar can be obtained therefrom polarizing at about 99.8 degrees.

While in describing our process, we have reierred specifically to the oxides of magnesium and calcium, it is to be clearly understood that this is not intended as a limitation. -The oxides of other alkaline earthmetals may also be used,

although we have not'found them to be quite as effective.

This completes the description of our present invention. It will be noted from all of the fore-.

going that we have provided a simple and inexpensively practiced process whereby we are able to obtain a highly purified, decolorized and deodorized sugar-containing liquid directly from be used, but it is desirable that it should be dry and in a finely powdered condition, and as free as possible from carbonate.

With the above methods as examples, other procedures can be used to give similar results, and such procedures will be obvious to those familiar with the art.

This mixture of compounds is added to the liquid to be purified, which, as indicated, may be cane or other sugar-bearing plant juice, fruit juice, a raw sugar melt, or a washed raw sugar melt. The amount added should be from about 1% to about 1.25%, based on the weight of the total sugar solids in the starting liquid, or an amount sufllcient to result in a liquid having a pH of about.10.00, or slightly higher.

It is preferred that the sugar-containing liquid be at room temperature during the addition of the magnesium-calcium combination, and it should be well stirred.

The liquid is then heated to from about 79 degrees to about 85 degrees C., the temperature being maintained at maximum for about 10 minutes. Within this range, and for such a time interval, no darkening occurs, and the precipitate obtained, which is flocculent and bulky, filters "well. The liquid is settled and decanted, the muds are filtered, and the filtrate added to the clear cane and other sugar-bearing plant juices, from fruit juices, from raw sugar melts, and from washed raw sugar melts.

Advantages or our present invention, in addition to those specifically referred to herein. will readily occur to those skilled in the art to which the same relates.

We claim:

-1. The method of treating a sugarrcontaining liquid which includes the steps of: adding to said liquid from about 1% toabout 1.25%, based on the weight of thetotal sugar solids in said liquid, of a mixture of the oxides of' magnesium and calcium; said oxide of magnesium constituting irom about 50% to about 10% of saidmixture; removing from the liquid the resulting precipitate; and thereafter adjusting the pH of the liquid substantially to neutrality.

2. The method of treating a sugar-containing liquid which includes the steps of: adding to said liquid from about 1% to about 1.25%, based on the weight of the total sugar solids in said liquid, of a mixture or the oxide and hydroxide of magnesium, and the oxide of calcium; said magnesium oxide and hydroxide constituting from about 50% to about 70% of said mixture,,a.n d said hydroxide constituting from about 2% to about 35% of the magnesium oxide-hydroxide combination; removing from the liquid the resulting precipitate; and thereafter adjusting the pH of the liquid substantially to neutrality.

3. The method of treating a sugar-containing liquid which includes the steps 0!: adding to said liquid 9. sufllcient quantity of a mixture of the oxide and hydroxide of magnesium, and the oxide of calcium to bring the pHoi said liquid to from about 10.00 to about 10.5; said magnesium oxide and hydroxide constituting from about 50%, to

magnesium oxide-hydroxide combination; heating the liquid to from about 79 degrees to about 85 degrees 0.; removing from the liquid the resulting precipitate: and thereafter adjusting the pH 01' the liquid substantially to neutrality.

4. The method of treating a sugar-containing liquid which includes the steps of: adding to said liquid from about 1% to about 1.25%, based on the weight oi. the total sugar solids in said liquid, of a mixture of the oxides of magnesium and calcium; said oxide of magnesium constituting from about 50% to about 70% of said mixture; removing from the liquid the resulting precipitate; adding phosphoric acid to the liquid to adjust the pH thereof to from about 6.9 to about 7.3; heating the liquid to about 83 degrees 0.; and removing irom the liquid the resulting precipitate.

5. The method of treating a sugar-containing liquid which includes the steps of: adding to said liquid from about 1% to about 1.25%, based on the weight of the total sugar solids in said liquid, of a mixture of the oxide and hydroxide of magnesium, and the oxide of calcium; said magnesium oxide and hydroxide constituting from about 50% to about 70% of said mixture, and said hydroxide constituting from about 2% toabout 35% of the magnesium oxide-hydroxide combination; removing from the liquid the resulting precipitate; adding phosphoric acid to the liquid to adjust the pH thereof to from about 6.9 to about 7.3; heating the liquid to about 83 degrees 0.; and removing from the liquid the resulting precipitate.

6. The method or treating a; sugar-containing liquid which includes the steps of: adding to'said liquid from about 1% to about 1.25%. based n the weight of the total sugar solids in said liquid, of a mixture of the oxide and hydroxide of magnesium, and the oxide of calcium; said magnesium oxide and hydroxide constituting from about to about of said mixture, and said hydroxide constituting from about 2% to about 35% of the magnesium oxide-hydroxide combination; heating the liquid to from about 79 degrees to about degrees 0.; removing from the liquid the resulting precipitate; adding phosphoric acid to the liquid to adjust the pH thereof to from about 6.9 to about 7.3; again heating the liquid to about 83 degrees (2.; and again removing from the liquid the resulting precipitate.

JOHN J. NAUGLE.

LEONARD WICKENDEN.

REFERENCES CITED The following references are of record in the file of this patent:

UNITED STATES PATENTS Number Name Date 517,820 Kolbig Apr. 3, 1894 518,538 Tiemann Apr. 17, 1894 1,052,113 Wiese Feb. 4, 1913 1,233,919 Rogan July 17, 1917 2,071,776 Teatini Feb. 23, 1937 2,340,128 Kent Jan. 25, 1944 FOREIGN PATENTS Number Country Date Great Britain 1877 

